CN106186048B - A kind of preparation method of the hierarchy indium oxide microballoon of cube composition - Google Patents
A kind of preparation method of the hierarchy indium oxide microballoon of cube composition Download PDFInfo
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- CN106186048B CN106186048B CN201610571609.3A CN201610571609A CN106186048B CN 106186048 B CN106186048 B CN 106186048B CN 201610571609 A CN201610571609 A CN 201610571609A CN 106186048 B CN106186048 B CN 106186048B
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention provides a kind of preparation method of the hierarchy indium oxide microballoon of cube composition.The preparation method is specifically included：Using inidum chloride and acetamide as raw material, using citric acid as surfactant, through hydro-thermal reaction, calcination processing, the indium oxide microballoon with hierarchy being made up of cube is obtained.This method simple production process, cost is than relatively low, and gained indium oxide can be as gas sensitive, because with hierarchy, material can obtain high sensitivity.
Description
Technical field
The present invention relates to a kind of preparation method of the hierarchy indium oxide microballoon of cube composition, belong to advanced nanometer work(
Can material preparation process technical field.
Background technology
The main tool of current detection of gas analysis has gas-chromatography, infrared gas analyser etc. than relatively large instrument,
But these instrument common problems have, and price is high, carries inconvenience, be difficult to carry out field monitoring etc., it is therefore desirable to develop
Superior performance, detection of gas material with low cost, and produce and some specific gas can at any time be detected, with just
Take the gas sensor of formula, high performance nature.Due to metal oxide semiconductor gas sensor have higher sensitivity, compared with
Fast response recovery time, circuit and many merits such as simple to operate, cheap, and be widely used medical treatment, aviation,
Life, gas discharge the every field such as detection at home.The research and development of conductor oxidate gas sensor have one so far
The history of section some time, wherein research emphasis are their sensitive performance of raising, especially sensitivity and selectivity.In2O3
It is a kind of new gas sensitive, some researchers is had at present and have been relevant In2O3Research as gas sensitive.In gas
In the detection method of body, because resistive memory gas sensor has, gas is applied widely, sensitivity is high, price is low
It is honest and clean, the advantages of make simple and with highly important status.In2O3As a kind of new gas sensitive, with SnO2、ZnO、
Fe2O3Deng traditional gas sensitive contrast, have the advantage that：Energy gap is wider, resistivity is small and relatively higher catalytic activity
Deng.In2O3Gas sensor can apply to the real-time prison of inflammable and explosive, toxic and harmful gas detection, alarm and environmental quality
The fields such as control.
In2O3The pattern and structure of material are to influence the principal element of its air-sensitive performance, and many scientific research personnel are directed in system
Its pattern and structure, or exploitation new construction is controlled to realize the raising of performance during standby.In the past few years, divide
Level material especially micro/nano structure is of great interest, mainly because its it is potential in optics, it is electronics, magnetics, bionical
The advantageous property for the application aspect learned and be catalyzed.It is used as important grading material, the In of different-shape2O3Micro/nano structure
In these years also there are many development.Jiang et al. are reported by hydro-thermal method and are combined the annealing process of InOOH presomas
To synthesize classification In2O3Microballoon.In recent years, three-dimensional hierarchical structure is increasingly becoming the focus of gas sensitive research field, with classification
The oxide-based nanomaterial of structure by with high surface area and the regularly arranged nano-pore structure for being not susceptible to reunite, thus
It is considered as very promising gas sensitive.China is for In2O3It is scarcely out of swaddling-clothes in terms of the research and processing of material,
In2O3Base research in nanotechnology is concentrated mainly on last decade, therefore also many problems need in depth to study.Therefore, high property is explored
Can In2O3Base functional material be one still need to solution the problem of.
The content of the invention
It is an object of the present invention to overcome the deficiencies in the prior art, there is provided the hierarchy oxidation that a kind of cube is constituted
The preparation method of indium microballoon.Low with cost, simple production process, yield is high, non-environmental-pollution, it is easy to which industrialization is extensive raw
The characteristics of production.The sensitivity of the hierarchy indium oxide gas sensitive of gained cube composition is largely increased, available for gas
The fields such as body sensor.Realizing the technical scheme of the object of the invention is：A kind of hierarchy indium oxide microballoon of cube composition
Preparation method, it is characterised in that：It is anti-through hydro-thermal using citric acid as surfactant using inidum chloride and acetamide as raw material
Should, calcination processing, obtain the indium oxide microballoon with hierarchy being made up of cube.This method simple production process, into
This is than relatively low, and gained indium oxide can be as gas sensitive, because with hierarchy, material can obtain high sensitivity.This method
Simple production process, gained indium oxide gas sensitive has hierarchy, so as to obtain highly sensitive new gas sensitive.Tool
Body synthesis step is as follows：
（1）A certain amount of inidum chloride, acetamide and citric acid are weighed, is dissolved in deionized water, wherein the concentration of inidum chloride
For 0.02-0.05 mol/L, the concentration of acetamide is 0.02-0.08 mol/L, and the concentration of citric acid is 0.02-0.05 mol/
L, and control the mol ratio of inidum chloride and acetamide to be 1:The mol ratio of (1.5-2.5), inidum chloride and citric acid is 1:(1-
1.5)；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 170-
At a temperature of 220 DEG C, hydro-thermal reaction is carried out 8-24 hours, then the product utilization centrifuge after hydro-thermal reaction is subjected to separation of solid and liquid,
And gained solid product is repeatedly washed with deionized water and ethanol；
（3）By step（2）Gained solid product is positioned in drying box, 60 DEG C of dryings 24 hours, is subsequently placed in aluminum oxide
Crucible is put into Muffle furnace, is heat-treated 3 hours at 400-550 DEG C, obtains the indium oxide powder with hierarchy.
Brief description of the drawings
Fig. 1 is the XRD spectrum for the hierarchy indium oxide microballoon that cube is constituted.
Fig. 2 is the SEM figures for the hierarchy indium oxide microballoon that cube is constituted.
Fig. 3 is the hierarchy indium oxide microballoon FESEM figures that cube is constituted.
Fig. 4 is the TG-DSC collection of illustrative plates for the hierarchy indium oxide microballoon that cube is constituted.
Fig. 5 is cube is constituted under optimum operating voltage hierarchy indium oxide gas sensor to 10-500ppm first
The sensitivity curve figure of aldehyde gas.
The response recovery curve for the hierarchy indium oxide gas sensor that Fig. 6 constitutes for cube under optimum operating voltage
Figure.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementations
Example.
Embodiment 1
（1）A certain amount of inidum chloride, acetamide and citric acid are weighed, is dissolved in deionized water, wherein the concentration of inidum chloride
For 0.02 mol/L, the concentration of acetamide is 0.02 mol/L, and the concentration of citric acid is 0.02 mol/L, and control inidum chloride with
The mol ratio of acetamide is 1:1, the mol ratio of inidum chloride and citric acid is 1:1；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 170 DEG C
At a temperature of, carry out hydro-thermal reaction 8 hours, then the product utilization centrifuge after hydro-thermal reaction is subjected to separation of solid and liquid, and spend from
Sub- water and ethanol are repeatedly washed to gained solid product；
（3）By step（2）Gained solid product is positioned in drying box, 60 DEG C of dryings 24 hours, is subsequently placed in aluminum oxide
Crucible is put into Muffle furnace, is heat-treated 3 hours at 400 DEG C, obtains the indium oxide powder with hierarchy.
Embodiment 2
（1）A certain amount of inidum chloride, acetamide and citric acid are weighed, is dissolved in deionized water, wherein the concentration of inidum chloride
For 0.025 mol/L, the concentration of acetamide is 0.05 mol/L, and the concentration of citric acid is 0.025 mol/L, and controls inidum chloride
Mol ratio with acetamide is 1:2, the mol ratio of inidum chloride and citric acid is 1:1；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180 DEG C
At a temperature of, carry out hydro-thermal reaction 16 hours, then the product utilization centrifuge after hydro-thermal reaction is subjected to separation of solid and liquid, and spend from
Sub- water and ethanol are repeatedly washed to gained solid product；
（3）By step（2）Gained solid product is positioned in drying box, 60 DEG C of dryings 24 hours, is subsequently placed in aluminum oxide
Crucible is put into Muffle furnace, is heat-treated 3 hours at 400 DEG C, obtains the indium oxide powder with hierarchy.
Embodiment 3
（1）A certain amount of inidum chloride, acetamide and citric acid are weighed, is dissolved in deionized water, wherein the concentration of inidum chloride
For 0.025 mol/L, the concentration of acetamide is 0.05 mol/L, and the concentration of citric acid is 0.025 mol/L, and controls inidum chloride
Mol ratio with acetamide is 1:2, the mol ratio of inidum chloride and citric acid is 1:1；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180 DEG C
At a temperature of, carry out hydro-thermal reaction 24 hours, then the product utilization centrifuge after hydro-thermal reaction is subjected to separation of solid and liquid, and spend from
Sub- water and ethanol are repeatedly washed to gained solid product；
（3）By step（2）Gained solid product is positioned in drying box, 60 DEG C of dryings 24 hours, is subsequently placed in aluminum oxide
Crucible is put into Muffle furnace, is heat-treated 3 hours at 400 DEG C, obtains the indium oxide powder with hierarchy.
Embodiment 4
（1）A certain amount of inidum chloride, acetamide and citric acid are weighed, is dissolved in deionized water, wherein the concentration of inidum chloride
For 0.05 mol/L, the concentration of acetamide is 0.05 mol/L, and the concentration of citric acid is 0.025 mol/L, and controls inidum chloride
Mol ratio with acetamide is 1:1, the mol ratio of inidum chloride and citric acid is 2:1；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180 DEG C
At a temperature of, carry out hydro-thermal reaction 24 hours, then the product utilization centrifuge after hydro-thermal reaction is subjected to separation of solid and liquid, and spend from
Sub- water and ethanol are repeatedly washed to gained solid product；
（3）By step（2）Gained solid product is positioned in drying box, 60 DEG C of dryings 24 hours, is subsequently placed in aluminum oxide
Crucible is put into Muffle furnace, is heat-treated 3 hours at 400 DEG C, obtains the indium oxide powder with hierarchy.
Embodiment 5
（1）A certain amount of inidum chloride, acetamide and citric acid are weighed, is dissolved in deionized water, wherein the concentration of inidum chloride
For 0.025 mol/L, the concentration of acetamide is 0.05 mol/L, and the concentration of citric acid is 0.025 mol/L, and controls inidum chloride
Mol ratio with acetamide is 1:2, the mol ratio of inidum chloride and citric acid is 1:1；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 200 DEG C
At a temperature of, carry out hydro-thermal reaction 24 hours, then the product utilization centrifuge after hydro-thermal reaction is subjected to separation of solid and liquid, and spend from
Sub- water and ethanol are repeatedly washed to gained solid product；
（3）By step（2）Gained solid product is positioned in drying box, 60 DEG C of dryings 24 hours, is subsequently placed in aluminum oxide
Crucible is put into Muffle furnace, is heat-treated 3 hours at 400 DEG C, obtains the indium oxide powder with hierarchy.
Claims (1)
1. a kind of preparation method of the hierarchy indium oxide microballoon of cube composition, specific synthesis step is as follows：
（1）A certain amount of inidum chloride, acetamide and citric acid are weighed, is dissolved in deionized water, the concentration of wherein inidum chloride is
0.02-0.05 mol/L, the concentration of acetamide is 0.02-0.08 mol/L, and the concentration of citric acid is 0.02-0.05 mol/L,
And control the mol ratio of inidum chloride and acetamide to be 1:The mol ratio of (1.5-2.5), inidum chloride and citric acid is 1:(1-1.5)；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 170-220 DEG C
At a temperature of, carry out hydro-thermal reaction 8-24 hours, then the product utilization centrifuge after hydro-thermal reaction is subjected to separation of solid and liquid, and spend
Ionized water and ethanol are repeatedly washed to gained solid product；
（3）By step（2）Gained solid product is positioned in drying box, 60 DEG C of dryings 24 hours, is subsequently placed in alumina crucible
Muffle furnace is put into, is heat-treated 3 hours at 400-550 DEG C, obtains the indium oxide powder with hierarchy.
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| CN107140682B (en) * | 2017-06-12 | 2019-03-01 | 吉林大学 | A kind of the indium oxide powder and its low-temperature hydro-thermal synthesis of morphology controllable |
| CN107215889B (en) * | 2017-06-28 | 2019-01-04 | 济南大学 | A kind of preparation method of porous structure indium oxide cube gas sensitive |
| CN107215890A (en) * | 2017-06-28 | 2017-09-29 | 济南大学 | A kind of preparation method of cubic nanostructures indium oxide gas sensitive |
| CN110642287B (en) * | 2019-10-08 | 2022-01-07 | 济南大学 | Cubic phase In2O3Method for synthesizing micro/nano sphere structure |
| CN111111639B (en) * | 2020-01-15 | 2023-06-16 | 西安建筑科技大学 | ZnO/InOOH heterogeneous Z-type photocatalytic material and preparation method thereof |
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| CN101117236B (en) * | 2007-07-25 | 2012-08-08 | 中国科学院上海硅酸盐研究所 | Method for preparing crystal system controlled indium oxide powder |
| CN101927146B (en) * | 2009-06-23 | 2012-08-22 | 玉林师范学院 | Method for preparing In2O3 nano monocrystalline self-assembly microspheres |
| CN102826593A (en) * | 2012-09-11 | 2012-12-19 | 电子科技大学 | Preparation method for indium oxide nanometer material |
| CN103183374B (en) * | 2013-03-13 | 2014-10-01 | 济南大学 | Method for preparing monodisperse indium oxide nanometer porous microsphere |
| CN104229871A (en) * | 2014-06-24 | 2014-12-24 | 济南大学 | Preparation method of flower type indium oxide gas-sensitive material with hierarchical structure |
| CN105271370B (en) * | 2015-10-07 | 2017-01-25 | 济南大学 | Preparation method of hierarchical structured indium oxide hollow tubular gas-sensitive material |
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